CN1552497A - Ultramicroelement gas phase chromatothermography separating method and apparatus thereof - Google Patents
Ultramicroelement gas phase chromatothermography separating method and apparatus thereof Download PDFInfo
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- CN1552497A CN1552497A CNA031343538A CN03134353A CN1552497A CN 1552497 A CN1552497 A CN 1552497A CN A031343538 A CNA031343538 A CN A031343538A CN 03134353 A CN03134353 A CN 03134353A CN 1552497 A CN1552497 A CN 1552497A
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- chromatothermography
- gas phase
- ultramicro
- target
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Abstract
A gas-phase thermal chromatographic method and equipment for separating ultratrace elements features that after a lead target is heated in target furnace under protection of inertial gas and then bombarded by C12 beams in a vacuum environment, the trace elements released from lead target are cooled in a long delivery tube by a predefined temp gradient and then collected by a collector. Its advantages are high sensitivity and high effect.
Description
Technical field:
The present invention relates generally to the separation method of ultramicro-element, relates in particular to ultramicro-element gas phase chromatothermography separation method and device.
Background technology:
The conventional method that the gas phase chromatothermography is separated is the multiple low boiling element mixture that is gas phase, the transfer tube that has the negative temperature gradient distribution in weak gas flow drive lower edge one transports, and can be deposited on the diverse location of transfer tube inwall according to the different adiabatic condensation temperature of each element.But,, only manage to make it from metallic carrier, to deviate from as separating the element that is included in the solid metal block.As the ultramicro-element in the reguline metal is carried out high purity separation and with high efficiency with it collection, be the target that the basic skills of existing gas phase chromatothermography isolation technics still can't realize.
Summary of the invention:
The objective of the invention is to avoid the deficiencies in the prior art part and a kind of ultramicro-element gas phase chromatothermography separation method and separator are provided.
Purpose of the present invention can be by realizing by the following technical solutions: a kind of ultramicro-element gas phase chromatothermography separation method includes 2 * 10
-3-5 * 10
-4In the mmHg vacuum environment, by
12C bundle bombardment lead target plate (1), its main feature is also to include lead target plate (1) to heat in target stove (3), and imports faint inert protective gas; The trace element that lead target plate after the heating (1) volatilizes cools off by the thermograde of setting through longer transmission pipe (10); Gatherer (11) is collected trace element.
The He that the faint inert protective gas flow of input is 1-10ml/min makes vacuum environment reach 2 * 10
-3-5 * 10
-4MmHg.The protection of faint inert gas flow, the possibility of having exempted burning becomes the important foundation of efficient separation and collection.The heating-up temperature of described target stove (3) is 700-780 ℃; The thermograde of longer transmission pipe (10) is+700-30 ℃; The collection temperature of gatherer (11) is-10--30 ℃.
Ultramicro-element gas phase chromatothermography separator of the present invention includes shell (16), vavuum pump (17), and its main feature is also to include target stove (3), is provided with the graphite box (2) of placing lead target plate (1) in it; Target stove (3) communicates with longer transmission pipe (10), which is provided with to measure thermocouple (5); Longer transmission pipe (10) is provided with measures thermocouple (15), and its end is provided with gatherer (11) and refrigerating plant (12).
Described ultramicro-element gas phase chromatothermography separator is provided with the air inlet hair suction pipe (6) that feeds the inert protective gas helium in the target stove (3), it is connected with the tolerance control needle-valve (7) that shell (16) is provided with.Target stove (3) is included in the heater (3-1) that is provided with the tungsten filament coiling in the body of heater (3-2), and the material of body of heater (3-2) is a boron nitride.Be provided with stainless steel sleeve (19) or stainless steel shielding plate in the outside of target stove (3).The thermal-radiating effective shielding of body of heater adds the accurate measurement and the control of transfer tube cold-point temperature, has guaranteed the steady operation of chromatothermography pipe.The accurate measurement of the design of efficient heating stove and heating cabinet temperature and control have guaranteed trace element deviating from and separate with the success of high melting-point impurity from the bulk metal carrier.
Described refrigerating plant (12) includes liquid nitrogen (14), red copper is bathed rod (13), air ring (12-1) or refrigerator.Control liquid nitrogen surface height remains on-30--10 ℃ the transfer tube cold-point temperature.
Ultramicro-element gas phase chromatothermography separator of the present invention is provided with quartz fibre filler (8) at the interface of longer transmission pipe (10) and target stove (3), and its effect is to cause entering gas to produce diffuse scattering, and changing original directed movement is the diffuse scattering campaign.The inwall of longer transmission pipe (10) is provided with tantalum paper tinsel liner (9), and its length is 50-80cm.
Gatherer carrier in the gatherer (11) is Ag
2O
3Powder or Au paper tinsel.
The invention has the beneficial effects as follows:
The present invention be applicable to ultramicro-element (be separated pantogen subnumber with the ratio of the metal derby carrier atomicity that can melt at 1: 10
16To 1: 10
12Between) high sensitivity, efficient gas phase chromatothermography separate.
2. be particularly suitable for the separation and the collection of Mercury-197, have quick, highly sensitive, characteristics of high efficiency.
Description of drawings:
Fig. 1 looks generalized section for the master of the embodiment of the invention 2.
The specific embodiment:
Be described in further detail below in conjunction with the most preferred embodiment shown in the accompanying drawing:
Embodiment 1: a kind of ultramicron mercury element gas phase chromatothermography separation method, and 2 * 10
-3-5 * 10
-4In the mmHg vacuum environment, will
12The lead target plate 1 of C bundle bombardment heats in target stove 3, and heating-up temperature is 700-720 ℃.And import faint inert protective gas He, flow is 5ml/min.The trace element that lead target plate 1 after the fusing volatilizes through longer transmission pipe 10 by the thermograde of setting is+700-30 ℃ cooling; Gatherer 11 is collected trace element.The collection temperature of gatherer 11 is-10--30 ℃.
203The collection efficiency that the Hg tracer method is demarcated the mercury element product can reach more than 85%.Highly purified object element is collected with high efficiency.
Said method, the mercury element product that the isolated nuclei reaction generates from the lead target plate of being crossed by heavy ion irradiation in the laboratory is successful especially.The inventor at two kinds of new nucleic mercury-208 of mercury element, successfully uses and has verified the present invention in the first observed of mercury-209.Because mercury-208 (
208Hg) isotope can only be synthesized with atomic weak amount in nuclear process and (generate cross section about 1 * 10
-30Cm
2), and the product of association simultaneously in nuclear reaction is distributed in tens kinds of elements; Simultaneously, also to guarantee the not reason time delay of separating and decay of Mercury-197 isotope, require disengaging time short as much as possible.Under these conditions, the solid metal carrier melts, and object element is deviate from from metallic carrier.The ratio of separated mercury element atomicity and fusible metal derby carrier atomicity was at 1: 10
16To 1: 10
12Between, and can separate with simultaneous other impurity highly selective in the carrier, decontamination factor can reach 10
3-10
5
Embodiment 2: Fig. 1 looks generalized section for the master of the embodiment of the invention 2; A kind of ultramicro-element gas phase chromatothermography separator has shell 16, vavuum pump 17, and target stove 3 is provided with the graphite box 2 of placing lead target plate 1 in it.Target stove 3 communicates with longer transmission pipe 10, which is provided with to measure thermocouple 5.Longer transmission pipe 10 is provided with measures thermocouple 15, and its end is provided with gatherer 11 and refrigerating plant 12.Refrigerating plant 12 is made up of liquid nitrogen 14, red copper bath rod 13, air ring 12-1.Control liquid nitrogen surface height remains on-30--10 ℃ the transfer tube cold-point temperature.Be provided with the air inlet hair suction pipe 6 that feeds the inert protective gas helium in the target stove 3, it is connected with the tolerance control needle-valve 7 that shell 16 is provided with.Target stove (3) is provided with the heater 3-1 of tungsten filament coiling in body of heater 3-2, the material of body of heater 3-2 is a boron nitride.Be provided with stainless steel sleeve 19 in the outside of target stove 3.Interface at longer transmission pipe 10 and target stove 3 is provided with quartz fibre filler 8, and its inside pipe wall is provided with tantalum paper tinsel liner 9, and its length is 60-70cm.Collection carrier in the gatherer 11 is Ag
2O
3Powder.
During use, 2 * 10
-5-5 * 10
-6In the mmHg vacuum environment, by
12C bundle bombardment lead target plate 1, irradiation continues 3 hours.Then lead target plate 1 is put into the graphite box 2 of ultramicro-element gas phase chromatothermography separator, 2 * 10
-3-5 * 10
-4In the mmHg vacuum environment, heating in target stove 3, heating-up temperature is 700-720 ℃.By tolerance control needle-valve 7, hair suction pipe 6 input flow rates is the faint inert protective gas He of 5ml/min.Solid metal carrier lead target plate 1 melts, and trace element is deviate from from metallic carrier, and the interface quartz fibre filler 8 by target stove 3 enters longer transmission pipe 10.End at longer transmission pipe 10 is provided with refrigerating plant 12, and control liquid nitrogen surface height remains on-30--10 ℃ the transfer tube cold-point temperature.Owing to be provided with the shielding of the tantalum paper tinsel liner 9 that is provided with on stainless steel sleeve 19 and longer transmission pipe 10 inside pipe walls in the outside of target stove 3,, guaranteed the collection temperature of gatherer 11 so longer transmission pipe 10 forms negative temperature gradient.Collection carrier in the gatherer 11 is Ag
2O
3Powder.
Claims (10)
1. a ultramicro-element gas phase chromatothermography separation method includes 2 * 10
-3-5 * 10
-4In the mmHg vacuum environment, by
12C bundle bombardment lead target plate (1) is characterized in that also including lead target plate (1) and heats in target stove (3), and imports faint inert protective gas; The trace element that lead target plate after the heating (1) volatilizes cools off by the thermograde of setting through longer transmission pipe (10); Gatherer (11) is collected trace element.
2. ultramicro-element gas phase chromatothermography separation method as claimed in claim 1, the He that the faint inert protective gas flow that it is characterized in that also including described input is 1-10ml/min; The heating-up temperature of described target stove (3) is 700-780 ℃; The thermograde of longer transmission pipe (10) is+700--30 ℃; The collection temperature of gatherer (11) is-10--30 ℃.
3. a kind of ultramicro-element gas phase chromatothermography separator as claimed in claim 1 includes shell (16), and vavuum pump (17) is characterized in that also including target stove (3), is provided with the graphite box (2) of placing lead target plate (1) in it; Target stove (3) communicates with longer transmission pipe (10), which is provided with to measure thermocouple (5); Longer transmission pipe (10) is provided with measures thermocouple (15), and its end is provided with gatherer (11) and refrigerating plant (12).
4. ultramicro-element gas phase chromatothermography separator as claimed in claim 3 is characterized in that also comprising being provided with the air inlet hair suction pipe (6) that feeds the inert protective gas helium in the target stove (3) that it is connected with the tolerance control needle-valve (7) that shell (16) is provided with.
5. as claim 3,4 described ultramicro-element gas phase chromatothermography separators, it is characterized in that target stove (3) is included in the heater (3-1) that is provided with the tungsten filament coiling in the body of heater (3-2).
6. ultramicro-element gas phase chromatothermography separator as claimed in claim 5, the material that it is characterized in that body of heater (3-2) is a boron nitride.
7. ultramicro-element gas phase chromatothermography separator as claimed in claim 6 is characterized in that being provided with stainless steel sleeve (19) or stainless steel in the outside of target stove (3) shields plate.
8. ultramicro-element gas phase chromatothermography separator as claimed in claim 7 is characterized in that refrigerating plant (12) includes liquid nitrogen (14), red copper is bathed rod (13), air ring (12-1) or refrigerator.
9. ultramicro-element gas phase chromatothermography separator as claimed in claim 8 is characterized in that being provided with quartz fibre filler (8) at the interface of longer transmission pipe (10) and target stove (3), and its inside pipe wall is provided with tantalum paper tinsel liner (9), and its length is 50-80cm.
10. ultramicro-element gas phase chromatothermography separator as claimed in claim 9 is characterized in that the collection carrier in the gatherer (11) is Ag
2O
3Powder or Au paper tinsel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031343538A CN1552497A (en) | 2003-05-31 | 2003-05-31 | Ultramicroelement gas phase chromatothermography separating method and apparatus thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031343538A CN1552497A (en) | 2003-05-31 | 2003-05-31 | Ultramicroelement gas phase chromatothermography separating method and apparatus thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1552497A true CN1552497A (en) | 2004-12-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA031343538A Pending CN1552497A (en) | 2003-05-31 | 2003-05-31 | Ultramicroelement gas phase chromatothermography separating method and apparatus thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102974119A (en) * | 2012-12-18 | 2013-03-20 | 华东理工大学 | Gas condensation and grading device and application method thereof |
| CN104923077A (en) * | 2014-03-17 | 2015-09-23 | 住友重机械工业株式会社 | Radioactive isotope refining device and radioactive isotope refining method |
-
2003
- 2003-05-31 CN CNA031343538A patent/CN1552497A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102974119A (en) * | 2012-12-18 | 2013-03-20 | 华东理工大学 | Gas condensation and grading device and application method thereof |
| CN102974119B (en) * | 2012-12-18 | 2015-04-08 | 华东理工大学 | Gas condensation and grading device and application method thereof |
| CN104923077A (en) * | 2014-03-17 | 2015-09-23 | 住友重机械工业株式会社 | Radioactive isotope refining device and radioactive isotope refining method |
| JP2015175777A (en) * | 2014-03-17 | 2015-10-05 | 住友重機械工業株式会社 | Refiner of radioisotope, and refining method of radioisotope |
| CN104923077B (en) * | 2014-03-17 | 2017-06-13 | 住友重机械工业株式会社 | Radioisotopic refining plant and radioisotopic process for purification |
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